Separation and purification methods of highly purified antiviral active components in artichoke
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A technology for separation and purification of antiviral activity, applied in the field of separation and purification of high-purity antiviral active components in artichokes, can solve the problems of low recovery rate, high cost, time-consuming and laborious, etc., and achieve the effect of large separation capacity and strong performance
Inactive Publication Date: 2010-04-07
CENT SOUTH UNIV
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These methods are complicated in steps, time-consuming and laborious, and the recovery rate is low, the cost is high, and they are not suitable for industrialization.
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[0030] 1. Dried the whole artichoke at 50°C and crushed. Take 200g of crude drug, put it in a 2000mL round bottom flask, add 1600mL of 75% ethanol, reflux extraction 3 times, each time for 2h, filter, combine the filtrates, concentrate under reduced pressure until no alcohol smell, and recover the organic solvent. The concentrated solution is subjected to D101 macroporous adsorption resin column chromatography, washed with water until it has no alcohol smell, and then eluted with 20% and 40% ethanol aqueous solution in sequence, and the 40% ethanol eluate is collected and concentrated under reduced pressure until it is alcohol-free smell, add ethanol until the alcohol content is 80%, filter off the precipitate, take the supernatant and vacuum-dry to obtain the crude product of dicaffeoylquinic acid compounds. The crude product was separated and purified by high-speed countercurrent chromatography under the following conditions: rotation speed: 800rpm; solvent system: ethyl ace...
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Abstract
The invention discloses a method for efficiently separating and preparing highly purified antiviral active components (single caffeoylquinic acid compound and dicaffeoylquinic acid compound) in artichoke, mainly comprising the following steps: utilizing alcohol aqueous solution to extract fresh or dry artichoke, concentrating, carrying out column chromatographic separation, preparing crude extract rich in the antiviral active components, carrying out separation and purification on the crude extract by combing high speed counter-current chromatography with high preparative performance liquid chromatography, and finally adopting a recrystallization method for refining to obtain highly purified 1-O-caffeoylquinic acid, 3-O-caffeoylquinic acid, 4-O-caffeoylquinic acid, 5-O-caffeoylquinic acid, 1,3-di-O-caffeoylquinic acid, 1,5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, 3,4-di-O-caffeoyl quinine acid and 4,5-di-O-caffeoylquinic acid. The method is suitable for preparing highly purified monomer by utilizing various natural products or the extractives of the natural products containing one or more components containing the above caffeoylquinic acid compounds as raw materials, wherein the natural products or the extractives are obtained from various ways; and the method has simple steps, simple operation, high efficiency, low cost and large separating preparation quantity, is easy to repeat; and the purification of the caffeoylquinic acid compounds prepared by the method can be up to 98%.
Description
technical field [0001] The present invention relates to a separation and purification method of effective components in traditional Chinese medicine or natural products, mainly relates to a method for extracting and separating monomeric compounds from traditional Chinese medicine or natural products, in particular to a high-purity caffeoylquinic acid compound 1-O-coffee Caffeoylquinic acid, 3-O-caffeoylquinic acid, 4-O-caffeoylquinic acid, 5-O-caffeoylquinic acid, 1,3-di-O-caffeoylquinic acid, 1 , 5-di-O-caffeoylquinic acid, 3,5-di-O-caffeoylquinic acid, 3,4-di-O-caffeoylquinic acid and 4,5-di-O-caffeoylquinic acid A method for the separation and preparation of acylquinic acid. Background technique [0002] Artichoke (Cynara scolymus L., also known as artichoke, artichoke, artichoke, French lily, lotus lily) is a perennial herb of Compositae. Native to the Mediterranean coast. my country introduced the species from abroad in the 1990s, and it is currently planted on a lar...
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